1.青岛海关技术中心,山东 青岛 266500
2.宁波海关技术中心,浙江 宁波 315048
薛秋红,硕士,正高级工程师,研究方向:能源产品及环境分析,E-mail:xueqh2000@163.com
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刘一龙,薛秋红,管晓倩等.全二维气相色谱-飞行时间质谱法测定汽油中21种抗爆添加剂[J].分析测试学报,2022,41(02):196-203.
LIU Yi-long,XUE Qiu-hong,GUAN Xiao-qian,et al.Analysis of 21 Antiknock Additives in Gasoline by Comprehensive Two-dimensional Gas Chromatography-Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(02):196-203.
刘一龙,薛秋红,管晓倩等.全二维气相色谱-飞行时间质谱法测定汽油中21种抗爆添加剂[J].分析测试学报,2022,41(02):196-203. DOI: 10.19969/j.fxcsxb.21063001.
LIU Yi-long,XUE Qiu-hong,GUAN Xiao-qian,et al.Analysis of 21 Antiknock Additives in Gasoline by Comprehensive Two-dimensional Gas Chromatography-Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(02):196-203. DOI: 10.19969/j.fxcsxb.21063001.
应用全二维气相色谱-飞行时间质谱技术建立了汽油中21种抗爆添加剂的检测方法。对仪器分析条件和定量方式进行了优化,充分利用全二维色谱柱容量大和分离能力强的特点,实现了21种多类别抗爆添加剂的同时检测,其中包含醇类10种、醚类5种、酯类3种、胺类2种、酮类1种。应用加权最小二乘法进行定量,有效提升了低浓度样品的定量准确性。研究结果表明21种抗爆添加剂在50 ~ 10 000 mg/L质量浓度范围内线性关系良好,线性相关系数(,r,2,)均大于0.995;4个水平(0.5%、2.0%、5.0%、10.0%)下的加标回收率为91.1% ~ 109%,相对标准偏差(RSDs, ,n ,= 6)小于5.0%;方法的检出限(,S/N ,≥ 3)为0.000 4%~0.014 1%,定量下限(,S/N ,≥ 10)为0.001 4%~0.046 9%。该方法可以满足实际样品中抗爆添加剂的检测需要。
A comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry was established for the detection of 21 antiknock additives in gasoline.The instrument analysis conditions and quantitative parameters were optimized. Taking full advantage of the superiority in column capacity and separation ability of comprehensive two-dimensional gas chromatography,21 antiknock additives,including 10 alcohols,5 ethers,3 esters,2 amines and 1 ketone,were detected simultaneously.The quantitative accuracies for low concentration samples were improved by weighted least square method.Results showed that there were good linear relationships for 21 additives in the concentration range of 50-10 000 mg/L,with their correlation coefficients(,r,2,)greater than 0.995.The recoveries at four concentration levels of 0.5%,2.0%,5.0% and 10.0% ranged from 91.1% to 109%,with the relative standard deviations(RSDs, ,n ,= 6)less than 5.0%.The limits of detection(,S,/,N ,≥ 3)and the limits of quantification(,S,/,N ,≥ 10)were in the range of 0.000 4%-0.014 1% and 0.001 4%-0.046 9%,respectively.This method could satisfy the requirements for detection of antiknock additives in actual samples.
全二维气相色谱-飞行时间质谱汽油抗爆添加剂加权最小二乘法
comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometrygasolineantiknock additiveweighted least square method
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